CN104036911B - Magnetic material [Cu3Na2(ehbd)2(N3)6]nAnd synthetic method - Google Patents
Magnetic material [Cu3Na2(ehbd)2(N3)6]nAnd synthetic method Download PDFInfo
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Abstract
The invention discloses a kind of magnetic material [Cu3Na2(ehbd)2(N3)6]nAnd synthetic method.Magnetic material [Cu3Na2(ehbd)2(N3)6]nMolecular formula be：C18H18Cu3N18Na2O6Molecular weight is：819.13, Hehbd be the hydroxy benzaldehyde of 3 ethyoxyl 2.The analytically pure hydroxy benzaldehydes of 3 ethyoxyl 2 of 0.125 0.25g are dissolved in 10 20 milliliters of pure acetonitrile solutions of analysis, sequentially add 0.278 0.556g and analyze pure Cupric diperchlorate hexahydrate and the analytically pure sodium azide of 0.098 0.196g, addition is analyzed pure triethylamine and adjusted to pH=6.5 after stirring makes solution well mixed for 10 minutes, stirring, stand, filtering, washing, products C is obtained after being dried in air18H18Cu3N18Na2O6。[Cu3Na2(ehbd)2(N3)6]nMagnetic property：Ferromagnetic exchange be present between intermolecular copper ion, its general performance is ferromagnetism.The present invention has the advantages that technique is simple, cost is cheap, chemical constituent is easily controllable, reproducible and yield is high.
Description
Technical field
The present invention relates to a kind of magnetic material [Cu3Na2(ehbd)2(N3)6]n(Hehbd is 3- ethyoxyl -2- hydroxy benzenes first
Aldehyde) and synthetic method.
Background technology
Modem magnetic materials have been widely used among our life, such as permanent-magnet material is used as into motor, application
Core material in transformer, the magneto-optic disk used as memory, computer magnetic recording floppy disk etc..It can be said that magnetic
Material is closely related with informationization, automation, electromechanical integration, national defence, the every aspect of national economy.For complex magnetic
For material, it is its fast-developing foundation to explore mechanism caused by its magnetic and establish rational theoretical model.Set from molecule
Be included in hand, rationally cut molecular structure, both can economy quickly develop magnetic partner, can carry out functional group to it again repaiies
Decorations change its magnetic.As people are theoretical to magnetic and Coordinative Chemistry research is goed deep into, will synthesize more has practical valency
The coordination compound magnetic material of value, and the application of these coordination compound magnetic materials will be led in space flight, aviation, military project, information, superconduction etc.
Trigger a series of great technological innovations in domain.
The content of the invention
The purpose of the present invention is exactly to synthesize the excellent functional material of magnetic property for design, utilizes normal temperature solwution method to synthesize skill
Art synthesizes [Cu3Na2(ehbd)2(N3)6]n。
[Cu of the present invention3Na2(ehbd)2(N3)6]nMolecular formula be：C18H18Cu3N18Na2O6, molecular weight is：
819.13, Hehbd be 3- ethyoxyls-Benzaldehyde,2-hydroxy, and crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
[the Cu of table one3Na2(ehbd)2(N3)6]nCrystallographic parameter
[the Cu of table two3Na2(ehbd)2(N3)6]nBond distanceWith bond angle (°)
[Cu3Na2(ehbd)2(N3)6]nSynthetic method concretely comprise the following steps：
The analytically pure 3- ethyoxyls-Benzaldehyde,2-hydroxies of 0.125-0.25g are dissolved in 10-20 milliliters and analyze pure acetonitrile solution
In, sequentially add 0.278-0.556g and analyze pure Cupric diperchlorate hexahydrate and the analytically pure sodium azide of 0.098-0.196g,
Addition is analyzed pure triethylamine and adjusted to pH=6.5 after stirring makes solution well mixed for 10 minutes, after continuing stirring 20 minutes, by institute
Obtained mixed liquor is stood at room temperature, and black bulk crystals are obtained after three days, is filtered, and with the pure acetonitrile washes clean of analysis,
Product [Cu is obtained after being dried in air3Na2(ehbd)2(N3)6]n。
[Cu3Na2(ehbd)2(N3)6]nMagnetic property：Ferromagnetic exchange be present between intermolecular copper ion, its general performance
For ferromagnetism.
The present invention has the advantages that technique is simple, cost is cheap, chemical constituent is easily controllable, reproducible and yield is high.
Brief description of the drawings
Fig. 1 is the present invention [Cu3Na2(ehbd)2(N3)6]nStructure chart.
Fig. 2 is the present invention [Cu3Na2(ehbd)2(N3)6]n2D stratiform figures, for clarity, removing whole carbon atoms and portion
Divide nitrogen-atoms.
Fig. 3 is the present invention [Cu3Na2(ehbd)2(N3)6]nχM-T,χMT-T curve maps.
Fig. 4 is the present invention [Cu3Na2(ehbd)2(N3)6]nχM –1- T curve figure.
Embodiment
Embodiment 1：
[Cu of the present invention3Na2(ehbd)2(N3)6]nMolecular formula be：C18H18Cu3N18Na2O6
Molecular weight is：819.13.
[Cu3Na2(ehbd)2(N3)6]nSynthetic method concretely comprise the following steps：
(1) 0.125 gram of analytically pure 3- ethyoxyls-Benzaldehyde,2-hydroxy is dissolved in 10 milliliters of pure acetonitrile solutions of analysis,
Sequentially add 0.278g and analyze pure Cupric diperchlorate hexahydrate and the analytically pure sodium azide of 0.098g, and stir make within 10 minutes it is molten
The pure triethylamine of analysis is added after liquid is well mixed to adjust to pH=6.5, it is after continuing stirring 20 minutes, obtained mixed liquor is quiet
It is placed at room temperature, black bulk crystals is obtained after three days, filters, and with the pure acetonitrile washes clean of analysis, after being dried in air
Obtain product [Cu3Na2(ehbd)2(N3)6]n.Yield：124 milligrams, yield：60.7%.[Cu is determined by single crystal diffractometer3Na2
(ehbd)2(N3)6]nStructure, crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
(2) product [Cu for obtaining 0.0239 gram of step (1)3Na2(ehbd)2(N3)6]nIn Magnetic Test instrument after pulverizing
Upper carry out Magnetic Test, obtain Magnetic Test curve such as accompanying drawing 2,3, [Cu3Na2(ehbd)2(N3)6]nχ at room temperatureMT is
1.32cm3Kmol1, as temperature reduces, χMT gradually rises, and reaches maximum 1.52cm to 20K3Kmol-1, then drastically it is down to
0.84cm3Kmol-1.To χM-T,χMT-T curve obtain after analysis fitting the Lang De factors as 2.09, intermolecular copper ion it
Between magnetic exchange constant be 36.81cm-1, the magnetic exchange constant of intramolecular copper ion is：-20.22cm-1.And χM –1- T curve is abided by
From Curie-Weiss law, it is 11.04K, Curie constant 1.28cm that it, which is fitted, to obtain Wei Si constants3Kmol–1.Big and positive
Wei Si constants, intermolecular magnetic exchange constant and χMT-T curvilinear trends imply between copper ion ferromagnetic exchange be present, its general performance
For ferromagnetism.
Embodiment 2：
[Cu of the present invention3Na2(ehbd)2(N3)6]nMolecular formula be：C18H18Cu3N18Na2O6
Molecular weight is：819.13.
[Cu3Na2(ehbd)2(N3)6]nSynthetic method concretely comprise the following steps：
(1) 0.25 gram of analytically pure 3- ethyoxyls-Benzaldehyde,2-hydroxy is dissolved in 20 milliliters of analytically pure acetonitrile solutions,
The analytically pure Cupric diperchlorate hexahydrates of 0.556g and the analytically pure sodium azide of 0.196g are sequentially added, and stirring makes for 10 minutes
Analytically pure triethylamine is added after solution is well mixed to adjust to pH=6.5, after continuing stirring 20 minutes, by obtained mixing
Liquid is stood at room temperature, and black bulk crystals are obtained after three days, is filtered, and with pure acetonitrile washes clean is analyzed, is dried in the air in air
Product [Cu is obtained after dry3Na2(ehbd)2(N3)6]n。
(2) product [Cu for obtaining 0.0239 gram of step (1)3Na2(ehbd)2(N3)6]nIn Magnetic Test instrument after pulverizing
Upper carry out Magnetic Test, obtain Magnetic Test curve such as accompanying drawing 2,3, [Cu3Na2(ehbd)2(N3)6]nχ at room temperatureMT is
1.32cm3Kmol–1, as temperature reduces, χMT gradually rises, and reaches maximum 1.52cm to 20K3Kmol-1, then drastically drop
To 0.84cm3Kmol-1.To χM-T,χMT-T curve obtain after analysis fitting the Lang De factors as 2.09, intermolecular copper ion
Between magnetic exchange constant be 36.81cm-1, the magnetic exchange constant of intramolecular copper ion is：-20.22cm-1.And χM –1- T curve
Curie-Weiss law is deferred to, it is 11.04K, Curie constant 1.28cm that it, which is fitted, to obtain Wei Si constants3Kmol–1.It is big and just
Wei Si constants, intermolecular magnetic exchange constant and χMT-T curvilinear trends imply between copper ion ferromagnetic exchange be present, its overall table
It is now ferromagnetism.
Claims (1)
- A kind of 1. magnetic material [Cu3Na2(ehbd)2(N3)6]n, it is characterised in that [Cu3Na2(ehbd)2(N3)6]nMolecular formula is： C18H18Cu3N18 Na2O6, molecular weight is：819.13, Hehbd be 3- ethyoxyls-Benzaldehyde,2-hydroxy；[Cu3Na2(ehbd)2 (N3)6]nMagnetic property：(1) ferromagnetic exchange be present between intermolecular copper ion, its general performance is ferromagnetism；(2) [Cu3Na2 (ehbd)2(N3)6]nχ at room temperatureM TFor 1.32cm3 Kmol-1, as temperature reduces, χM TGradually rise, reach maximum to 20K The cm of value 1.523 Kmol-1, then drastically it is down to 0.84 cm3 Kmol-1；Rightχ M - T, χ M T – TCurve carries out analysis plan It is 2.09 that the Lang De factors are obtained after conjunction, and the magnetic exchange constant between intermolecular copper ion is 36.81cm-1, intramolecular copper ion Magnetic exchange constant is：-20.22cm-1；Andχ M –1 -TCurve defers to Curie-Weiss law, it is fitted to obtain Wei Si constants be 11.04K, Curie constant 1.28cm3Kmol–1；Big and positive Wei Si constants, intermolecular magnetic exchange constant and χM T-TCurve becomes Gesture implies between copper ion ferromagnetic exchange be present, and its general performance is ferromagnetism；[the Cu3Na2(ehbd)2(N3)6]nSynthetic method concretely comprise the following steps：The analytically pure 3- ethyoxyls-Benzaldehyde,2-hydroxies of 0.125-0.25g are dissolved in into 10-20 milliliters to analyze in pure acetonitrile solution, Sequentially add 0.278-0.556g and analyze pure Cupric diperchlorate hexahydrate and the analytically pure sodium azide of 0.098-0.196g, stirring Addition is analyzed pure triethylamine and adjusted to pH=6.5 after making within 10 minutes solution well mixed, will be made after continuing stirring 20 minutes Mixed liquor stand at room temperature, black bulk crystals are obtained after three days, are filtered, and with the pure acetonitrile washes cleans of analysis, in [Cu is obtained after being dried in air3Na2(ehbd)2(N3)6]n。
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| CN101418021A (en) * | 2008-11-05 | 2009-04-29 | 江苏科技大学 | Octcyano bimetal coordination polymer and preparation method thereof |
| EP2216083A2 (en) * | 2003-06-27 | 2010-08-11 | Invitrogen Dynal AS | Conjugates of magnetic polymer particles and carboxymethylated aspartic acid |
| CN103113876A (en) * | 2013-01-22 | 2013-05-22 | 中国科学院福建物质结构研究所 | Photochromic optomagnetic material |
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| EP2216083A2 (en) * | 2003-06-27 | 2010-08-11 | Invitrogen Dynal AS | Conjugates of magnetic polymer particles and carboxymethylated aspartic acid |
| CN101418021A (en) * | 2008-11-05 | 2009-04-29 | 江苏科技大学 | Octcyano bimetal coordination polymer and preparation method thereof |
| CN103113876A (en) * | 2013-01-22 | 2013-05-22 | 中国科学院福建物质结构研究所 | Photochromic optomagnetic material |
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| 3，5-二溴水杨醛缩邻苯二胺双希夫碱Cu(Ⅱ)配合物的合成及其晶体结构;丁国华等;《桂林理工大学学报》;20110228;第31卷(第1期);第106-109页 * |
| Synthesis and characterization of an amidinate-stabilized siladithiocarboxylate and its germanium(II) complex;Shu-Hua Zhang等;《Organometallics》;20110607;第30卷(第13期);第3686-3689页 * |
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